CN111363232B - Low-smoke halogen-free flame-retardant master batch and preparation method and application thereof - Google Patents
Low-smoke halogen-free flame-retardant master batch and preparation method and application thereof Download PDFInfo
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- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
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- C08J2431/00—Characterised by the use of copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an acyloxy radical of a saturated carboxylic acid, or carbonic acid, or of a haloformic acid
- C08J2431/02—Characterised by the use of omopolymers or copolymers of esters of monocarboxylic acids
- C08J2431/04—Homopolymers or copolymers of vinyl acetate
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- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/34—Heterocyclic compounds having nitrogen in the ring
- C08K5/3467—Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
- C08K5/3477—Six-membered rings
- C08K5/3492—Triazines
- C08K5/34928—Salts
Abstract
The invention discloses a low-smoke halogen-free flame-retardant master batch, a preparation method and application thereof, wherein the flame-retardant master batch comprises the following components in parts by mass: 60-80 parts of matrix resin, 20-40 parts of compatilizer, 400 parts of first flame retardant 250-one, 15-35 parts of second flame retardant and 3-6 parts of coupling agent, wherein the matrix resin is composed of EVM resin, EVA resin and POE resin according to the feeding mass ratio of 1.5-2.5: 1: 1.3-2.5, and the flame retardants comprise different first flame retardant and second flame retardant which are respectively selected from halogen-free flame retardants; the preparation method comprises the following steps: mixing the flame retardant and the coupling agent, then mixing with the rest components, and performing extrusion molding to obtain the flame retardant; the application comprises the following steps: a low-smoke halogen-free flame-retardant product containing the master batch; the low-smoke halogen-free flame-retardant master batch disclosed by the invention has the advantages of obvious improvement on flame retardance and strong compatibility, and can be suitable for preparing flame-retardant materials from various high polymer materials.
Description
Technical Field
The invention belongs to the technical field of flame retardance, and particularly relates to a low-smoke halogen-free flame-retardant master batch, and a preparation method and application thereof.
Background
The application of the high polymer material is more and more extensive, and the high polymer material plays an increasingly important role in national economy. However, most of polymer materials have better application performance, but have the disadvantage of easy combustion, thereby having great potential safety hazard, and generating smoke gas to different degrees while combusting, which causes environmental pollution.
At present, flame retardant performance of high polymer materials is generally improved by adding flame retardants in the prior art, but with increasingly strict social requirements on environmental protection, the conventional application of mature halogen flame retardants (which release smoke with extremely high toxicity and toxic and highly corrosive hydrogen halide gas during combustion) is gradually abandoned by people, and halogen-free flame retardants such as phosphorus flame retardants, nitrogen flame retardants, boron flame retardants, aluminum hydroxide, magnesium hydroxide and the like are selected. However, the application of these halogen-free flame retardants still has the following problems:
1. the processing process is complicated, the halogen-free flame retardant has a powder lifting phenomenon in the processing process, and the dust in the processing environment is large, so that the environment protection and the body health of operators are not facilitated;
2. the halogen-free flame retardant needs high filling amount to obtain better flame retardant effect, but the high filling amount brings about the problems that the dispersibility of the halogen-free flame retardant in a high molecular resin material is poor, the mechanical property and the like of a molding material are influenced to a certain extent, and the processing difficulty is increased.
In order to solve the above problems, some improved technical solutions are proposed in the prior art, for example, a flame retardant master batch is first prepared, and then the flame retardant master batch is compounded with a matrix resin to prepare a polymer material with a low smoke, zero halogen and flame retardant function.
For example, chinese patent No. CN101265410B discloses a multifunctional flame retardant masterbatch, which is prepared by properly mixing and processing a flame retardant and a polymer matrix, wherein the flame retardant masterbatch further comprises at least one rare earth surface treatment agent having a functional group for binding the flame retardant and a functional group for binding the polymer matrix, wherein the ratio of the rare earth surface treatment agent, the flame retardant and the polymer matrix is 0.5-10: 30-200: 100, respectively; wherein, the flame-retardant master batch also comprises more than one reinforcing agent and/or toughening agent; wherein the flame retardant is more than one halogen-free flame retardant selected from the following group of species: phosphorus flame retardants, nitrogen flame retardants, polymeric flame retardants, and inorganic hydroxide flame retardants; the reinforcing agent is an inorganic substance or whisker with a layered structure; the toughening agent is rubber, a thermoplastic elastomer and/or a crystal modifier. The patent treats the flame retardant and the polymer matrix by the rare earth surface treating agent and the like, so that the flame retardant master batch is uniformly dispersed, mixed and processed into the master batch type flame retardant master batch; however, although the flame retardance, mechanical property and processability of the flame retardant material are improved to a certain extent, firstly, the flame retardant addition amount of the flame retardant master batch is not enough, so that the flame retardant property of the flame retardant master batch of unit mass part on the material is improved to a limited extent, and secondly, the flame retardant master batch has insufficient compatibility, namely when the resin adopted for preparing the master batch is different from the polymer base material to be prepared, the resin is difficult to truly exert the functions of improving the flame retardance, the mechanical property and the processability, and the applicability of the resin is seriously hindered.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides the improved low-smoke halogen-free flame-retardant master batch which has obvious improved flame retardance and strong compatibility and can be suitable for preparing flame-retardant materials from various high polymer materials.
The invention also provides a preparation method of the low-smoke halogen-free flame-retardant master batch.
The invention also provides an application of the low-smoke halogen-free flame-retardant master batch in preparing low-smoke halogen-free flame-retardant products.
In order to achieve the purpose, the invention adopts a technical scheme that:
a low-smoke halogen-free flame-retardant master batch comprises the following components: the flame retardant comprises base resin and a flame retardant, wherein the base resin is composed of EVM resin, EVA resin and POE resin, the feeding mass ratio of the EVM resin to the EVA resin to the POE resin is 1.5-2.5: 1: 1.3-2.5, and the flame retardant comprises a first flame retardant and a second flame retardant which are respectively selected from halogen-free flame retardants and are different; the flame-retardant master batch also comprises a compatilizer and a coupling agent;
wherein, in the flame-retardant master batch, by mass: 60-80 parts of matrix resin, 20-40 parts of compatilizer, 400 parts of first flame retardant 250-35 parts of second flame retardant and 3-6 parts of coupling agent; the VA content in the EVM resin is more than 50%, the melt index of the EVA resin is 50-150g/10min, and the melt index of the POE resin is 2-5g/10 min.
According to some preferred aspects of the invention, the compatibilizer is one or both of a POE/LLDPE or EVA compatibilizer having a melt index of 1.5 to 3.5g/10 min.
According to some specific aspects of the invention, the POE/LLDPE compatibilizer can be available from tengyu under the designation Y196; the EVA compatibilizer may be available from tengyu under the designation Y199.
According to some preferred aspects of the present invention, the charging mass ratio of the EVM resin, the EVA resin and the POE resin is 1.8-2.2: 1: 1.4-2.0.
According to some specific and preferred aspects of the present invention, the first flame retardant is a combination of one or more selected from the group consisting of aluminum hydroxide, magnesium hydroxide, melamine phosphate and melamine cyanurate.
According to some specific and preferred aspects of the present invention, the second flame retardant is a combination of one or more selected from the group consisting of organic montmorillonite, silicone powder, a silicon-based flame retardant other than silicone powder, and zinc borate.
According to some specific aspects of the invention, the coupling agent is a combination of one or more selected from the group consisting of vinyltrimethoxysilane, vinyltriethoxysilane, and divinyltriaminopropyltrimethoxysilane.
According to some specific aspects of the invention, the flame-retardant master batch further comprises 2-10 parts of other auxiliary agents, wherein the other auxiliary agents are a combination of one or more selected from grafted polyethylene wax, an antioxidant (which can be antioxidant 1010, DLTP), a rheological agent, an ultraviolet ray resistant absorbent and a rat and ant resistant material.
The invention provides another technical scheme that: the preparation method of the low-smoke halogen-free flame-retardant master batch comprises the following steps: weighing the raw materials according to the formula ratio, putting the first flame retardant into a mixer for uniform mixing, spraying the coupling agent in the mixing process, uniformly spraying the coupling agent by using an atomizing device, stirring, adding the second flame retardant, and stirring to prepare a premix; adding the rest raw materials into a mixer, uniformly stirring with the premix, and then extruding and granulating; wherein, the extrusion temperature is: feeding at 60-100 ℃, melting section: 120 ℃ 140 ℃, die: 130 ℃ and 145 ℃.
The invention provides another technical scheme that: the low-smoke halogen-free flame-retardant product comprises a high-molecular resin matrix and the low-smoke halogen-free flame-retardant master batch.
According to some preferred and specific aspects of the present invention, in the low-smoke halogen-free flame-retardant product, the low-smoke halogen-free flame-retardant master batch accounts for 50 to 90% by mass of the raw material.
According to the invention, the low-smoke halogen-free flame-retardant master batch can be directly mixed with a common resin matrix to prepare a low-smoke halogen-free flame-retardant product, and can still realize better flame retardance, mechanical properties and extrusion processability without adding other additives.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
according to the invention, the specific EVM resin, the EVA resin with the specific melt index and the POE resin material are innovatively compounded to serve as the resin matrix, and a certain amount of compatilizer is combined, so that the flame-retardant master batch can be highly dispersed even if containing a high-content flame retardant, the secondary dispersion can better play the role of the flame retardant when a low-smoke halogen-free product is prepared, and the flowability is better during processing, so that the processing is facilitated; particularly, the flame-retardant master batch disclosed by the invention is endowed with excellent compatibility, namely for halogen-free flame-retardant products taking different high polymer materials as carrier resins, the flame-retardant master batch disclosed by the invention is excellent in compatibility with the flame-retardant master batch, so that a single master batch can be applied to different products conveniently and quickly, the effects of improving the flame retardance, the mechanical property and the processing property of the flame-retardant master batch can be exerted to the maximum extent, and the market prospect is excellent.
Detailed Description
The above-described scheme is further illustrated below with reference to specific examples; it is to be understood that these embodiments are provided to illustrate the general principles, essential features and advantages of the present invention, and the present invention is not limited in scope by the following embodiments; the implementation conditions used in the examples can be further adjusted according to specific requirements, and the implementation conditions not indicated are generally the conditions in routine experiments.
Not specifically illustrated in the following examples, all starting materials are commercially available or prepared by methods conventional in the art.
Examples 1 to 3.
The embodiments provide a low-smoke halogen-free flame-retardant master batch, and the raw materials and the dosage of the master batch are shown in table 1.
TABLE 1
The preparation method of the low-smoke halogen-free flame-retardant master batch comprises the following steps: weighing the raw materials according to the formula ratio, putting the first flame retardant into a mixer for uniform mixing, spraying the coupling agent in the mixing process, uniformly spraying the coupling agent by using an atomizing device, stirring, adding the second flame retardant, and stirring to prepare a premix; adding the rest raw materials into a mixer, uniformly stirring with the premix, and then extruding and granulating; wherein, the extrusion temperature is: feeding material at 80 +/-5 ℃, melting section: 130 ± 5 ℃, die head: 138. + -. 3 ℃.
Comparative example 1
The difference is essentially the same as example 1, except that no EVM resin is added to the matrix resin and the EVA resin content is adjusted accordingly.
Comparative example 2
The difference is essentially the same as example 1, except that no EVA resin is added to the matrix resin and the content of EVM resin is adjusted accordingly.
Comparative example 3
Basically, the same procedure as in example 1 was repeated, except that the POE resin was not added to the base resin, and the content of the EVA resin was adjusted accordingly.
Comparative example 4
Basically, the only difference from example 1 is that in the matrix resin: the feeding mass ratio of the EVM resin, the EVA resin and the POE resin is 1: 1.
Comparative example 5
Basically, the only difference from example 1 is that in the matrix resin: the melt indexes of the EVA resin and the POE resin are respectively 5g/10min and 1.0g/10 min.
Application examples 1 to 5 and application comparative examples 1 to 7
The following are resins commonly used in the art:
general resin 1: EVA;
resin 2 used: polyethylene resin PE;
resin 3: and (3) POE resin.
The following examples provide some products prepared by adding the above-mentioned low smoke zero halogen flame retardant masterbatch of examples 1-3 and comparative examples 1-5 to the above-mentioned conventional resin, and the specific raw materials and amounts are shown in tables 2 and 3.
Hereinafter, the master batches prepared in examples 1 to 3 are referred to as master batch 1, master batch 2 and master batch 3, respectively, and the master batches prepared in comparative examples 1 to 5 are referred to as master batch 1 ', master batch 2 ', master batch 3 ', master batch 4 ' and master batch 5 ', respectively.
TABLE 2
TABLE 3
Performance testing
The low smoke halogen-free flame retardant products prepared in the application examples 1 to 5 and the application comparative examples 1 to 7 were subjected to the following performance tests, and the specific results are shown in table 4.
TABLE 4
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. A low-smoke halogen-free flame-retardant master batch comprises the following components: the flame retardant comprises base resin and a flame retardant, and is characterized in that the base resin is composed of EVM resin, EVA resin and POE resin, the feeding mass ratio of the EVM resin to the EVA resin to the POE resin is 1.5-2.5: 1: 1.3-2.5, and the flame retardant comprises a first flame retardant and a second flame retardant which are respectively selected from halogen-free flame retardants and are different; the flame-retardant master batch also comprises a compatilizer and a coupling agent;
wherein, in the flame-retardant master batch, by mass: 60-80 parts of matrix resin, 20-40 parts of compatilizer, 400 parts of first flame retardant 250-35 parts of second flame retardant and 3-6 parts of coupling agent; the VA content in the EVM resin is more than 50%, the melt index of the EVA resin is 50-150g/10min, and the melt index of the POE resin is 2-5g/10 min;
the compatilizer is one or two of POE/LLDPE or EVA compatilizer with the melt index of 1.5-3.5g/10 min;
the first flame retardant is one or more of aluminum hydroxide, magnesium hydroxide, melamine phosphate and melamine cyanurate;
the second flame retardant is composed of organic montmorillonite, silicone powder, a silicon flame retardant except the silicone powder and zinc borate.
2. The low-smoke halogen-free flame-retardant master batch according to claim 1, wherein the charging mass ratio of the EVM resin, the EVA resin and the POE resin is 1.8-2.2: 1: 1.4-2.0.
3. The low smoke zero halogen flame retardant masterbatch according to claim 1, wherein the coupling agent is one or more selected from vinyltrimethoxysilane, vinyltriethoxysilane and divinyltriaminopropyltrimethoxysilane.
4. The low-smoke halogen-free flame-retardant master batch according to claim 1, further comprising 2-10 parts of other auxiliary agents, wherein the other auxiliary agents are one or more selected from grafted polyethylene wax, an antioxidant, a rheological agent, an ultraviolet ray resistant absorbent and a rat and ant resistant material.
5. A preparation method of the low smoke zero halogen flame retardant masterbatch according to any one of claims 1 to 4, wherein the preparation method comprises the following steps: weighing the raw materials according to the formula ratio, putting the first flame retardant into a mixer for uniform mixing, spraying the coupling agent in the mixing process, uniformly spraying the coupling agent by using an atomizing device, stirring, adding the second flame retardant, and stirring to prepare a premix; adding the rest raw materials into a mixer, uniformly stirring with the premix, and then extruding and granulating; wherein, the extrusion temperature is: feeding at 60-100 ℃, melting section: 120 ℃ 140 ℃, die: 130 ℃ and 145 ℃.
6. A low smoke zero halogen flame retardant product, the raw material of which comprises a high molecular resin matrix, characterized in that the raw material also comprises the low smoke zero halogen flame retardant master batch of any one of claims 1 to 4.
7. The low smoke zero halogen flame retardant product according to claim 6, characterized in that, in the low smoke zero halogen flame retardant product, the mass percentage of the low smoke zero halogen flame retardant master batch in the raw material is 50-90%.
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| CN103554637A (en) * | 2013-10-24 | 2014-02-05 | 宁波一舟塑胶有限公司 | High-elasticity wear-resistant low-smoke halogen-free flame-retardant injection molding material and preparation method thereof |
| CN104231420A (en) * | 2014-10-17 | 2014-12-24 | 上海至正道化高分子材料股份有限公司 | 105 DEG C Temperature-resist grade irradiation crosslinked low smoke halogen-free flame retardant insulation material and preparation method thereof |
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| KR100700798B1 (en) * | 2005-01-28 | 2007-03-27 | 엘에스전선 주식회사 | Composition for production flame retardant insulating material of halogen free type using nano-technology |
| CN103172918B (en) * | 2011-12-22 | 2016-12-07 | 上海杰事杰新材料(集团)股份有限公司 | A kind of fireproofing cable material without halide and preparation method thereof |
| CN104945728A (en) * | 2015-07-27 | 2015-09-30 | 上海至正道化高分子材料股份有限公司 | Low-smoke zero-halogen flame-retardant sheathing material for ultra-high-voltage cable and preparation method of sheathing material |
| CN105237885A (en) * | 2015-10-29 | 2016-01-13 | 宁波一舟塑胶有限公司 | High-filling low-smoke halogen-free flame-retardant polyolefin cable material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103554637A (en) * | 2013-10-24 | 2014-02-05 | 宁波一舟塑胶有限公司 | High-elasticity wear-resistant low-smoke halogen-free flame-retardant injection molding material and preparation method thereof |
| CN104231420A (en) * | 2014-10-17 | 2014-12-24 | 上海至正道化高分子材料股份有限公司 | 105 DEG C Temperature-resist grade irradiation crosslinked low smoke halogen-free flame retardant insulation material and preparation method thereof |
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